YL6500 Gas Chromatograph User Manual
YL6500 Gas Chromatograph User Manual
USER MANUAL
YL6500 GC
Contents
Chapter 1. Introduction ............................................................................................................................... 1
1-1. Gas Chromatography ...................................................................................................................... 1
1-2. Characters of the YL6500 GC ......................................................................................................... 2
1-2-1. Advanced Pneumatic Control (APC) .................................................................................... 3
1-2-2. Control of system .................................................................................................................. 4
1-2-3. Inlet ....................................................................................................................................... 5
1-2-4. Detector ................................................................................................................................ 5
1-2-5. Valve for gas sample ............................................................................................................ 5
1-2-6. Column oven......................................................................................................................... 5
1-3. Specifications of YL6500 GC .......................................................................................................... 6
Chapter 2. Installation ............................................................................................................................... 10
2-1. Environment for installation ........................................................................................................... 10
2-1-1. Place for installation ........................................................................................................... 10
2-1-2. Oven outlet ......................................................................................................................... 10
2-1-3. Safety sign ........................................................................................................................... 11
2-2. Check ............................................................................................................................................ 12
2-3. Power ............................................................................................................................................ 12
2-3-1. Power voltage ..................................................................................................................... 12
2-3-2. Power cable ........................................................................................................................ 12
2-2-3. Ground ................................................................................................................................ 12
2-3-4. Check the power ................................................................................................................. 12
2-4. Used gas ....................................................................................................................................... 13
2-4-1 Selection of gas ................................................................................................................... 13
2-4-2. Connection with a gas tube ................................................................................................ 14
Chapter 3. Screen ...................................................................................................................................... 16
3-1. Structure of Control Panel ............................................................................................................. 16
3-1-1. Home screen ...................................................................................................................... 16
3-1-2. Operation Key ..................................................................................................................... 20
3-1-3. LED Status .......................................................................................................................... 21
3-1-4. Screen settings and parameters entering .......................................................................... 21
3-2. SYSTEM Screen ........................................................................................................................... 22
3-2-1. Configuration ...................................................................................................................... 23
3-2-2. Information .......................................................................................................................... 24
3-2-4. Calibration........................................................................................................................... 29
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8-1-2. Connecting a power cable, a signal, and a remote line ................................................... 107
8-1-3. Preparing gas ................................................................................................................... 107
8-1-4. Preparing a column........................................................................................................... 107
8-2. Operation flow ............................................................................................................................. 108
8-3. Operating method of the equipment ........................................................................................... 109
8-3-1. FID analysis ...................................................................................................................... 109
8-3-2. TCD analysis ..................................................................................................................... 110
8-3-3.ECD analysis ...................................................................................................................... 110
8-3-4. Finishing operation after an analysis. ................................................................................ 111
Chapter 9. Maintenance .......................................................................................................................... 112
9-1. Introduction .................................................................................................................................. 112
9-1-1. Maintenance list ................................................................................................................. 112
9-1-2. Basic maintenance ............................................................................................................ 113
9-1-3. Trap maintenance .............................................................................................................. 114
9-2. Inlet .............................................................................................................................................. 115
9-2-1. Packed column inlet .......................................................................................................... 115
9-2-2. Capillary column inlet ........................................................................................................ 116
9-3. Oven ............................................................................................................................................. 118
9-3-1. Columm condition check and maintenance ....................................................................... 118
9-4. Detector ....................................................................................................................................... 120
9-4-1. Flame ionization detector (FID) ........................................................................................ 120
9-4-2. Thermal Conductivity Detector (TCD) .............................................................................. 123
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Chapter 1. Introduction
1-1. Gas Chromatography
In 1952, James and Martin devised Gas Chromatography(GC). After then, the technology has been
developed rapidly and has been used in many fields such as analytical chemistry and biochemistry. This
rapid progress has been made by introducing well developed capillary columns in it. These days, we can
easily analyze each component in a mixture by using GC-MS which uses Mass Spectrometer(MS) as a
detector.
Gas chromatography involves a sample vaporized and injected onto the head of a chromatographic
column. The sample is transported through the column by the flow of inert, gaseous mobile phase. The
separation is made during the transportation of the sample carried by gaseous mobile phase in the
column. The column itself contains a stationary phase. The mobile phase does not interact with the
molecules in the sample unlike other chromatography in GC analysis.
The carrier gas - the mobile phase - must be chemically inert. Commonly used gases are helium, argon,
and nitrogen. In gas-solid chromatography, the stationary phase is a solid which has wide surface area
and ability to absorb solutes for analysis. And the liquid stationary phase in gas-liquid chromatography is
chemically or physically coated on the surface of an inert solid which has wide surface area.
In gas chromatography, the partitioning of solutes between the mobile and stationary phases accounts for
the separation of solutes. In GC, partition ratio depends on vapor pressure of solutes, chemical characters
of each component, and an affinity for the stationary phase. Since these are all effected by temperature, it
is very important to choose the stationary phase of a column to get good results by optimizing analysis
condition. Also, temperature programming of a column is greatly important due to the same reason.
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The YL6500 GC is a rectangular box, approximately 605 mm width, 455 mm height, 550 mm depth. The
weight is 55 kg. It has a control panel for operation on the right side.
The control panel has a LCD screen for input of the operating conditions and display of the input data, a
LED for display of the status of the equipment, and a keypad for operation of the equipment and input of
variables. There are a power button below the control panel and a column oven on the left side of it. You
can open the oven by pushing a button which is below it.
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The Advanced Pneumatic Control system (APC) is designed to achieve the automatism and accuracy of
gas chromatography. It digitalizes the control of the volume of gas, which improves the accuracy of an
experiment and reduces the time for analysis.
You can use the APC in every inlets and detectors. Also, you can use various modes such as
Split/Splitless, Constant flow/pressure, and Ramped flow/pressure to obtain better results. The APC
controls the volume of hydrogen and air to reduce the exhaust of combustible gas – hydrogen - in a
detector like a Flame Ionization Detector (FID), which uses gas. This character of the APC improves the
safety and allows automatism like auto ignition.
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The YL6500 GC has a colorful touch screen (LCD) on the control panel which enables you to control
temperature of inlets, oven, and column and flow of gas. This graphic color LCD applies an intuitive
interface, large screen with the easy touch screen input to allow users to control GC in easy and
comfortable.
Also, YL6500 GC provides a function setting the auto operation according to the time. You can store all
equipment status, volume of flow, and temperature program as “Method-n”, and the feature of Time
Control enables you to save time. Besides these features, you can enjoy a lot of other functions for users.
More details will be described from Chapter 3.
Start/Stop button
Power button
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1-2-3. Inlet
The inlets of the YL6500 GC is designed for having no loss of sample and reaching the set temperature
rapidly. The maximum temperature for a packed column is 450 ℃, and for a capillary column is 400 ℃.
You can install various inlets such as Packed Inlet, Capillary Inlet, and On-Column Inlet. The maximum
number of inlets to be installed on one GC is three.
1-2-4. Detector
In the YL6500 GC, you can equip various detectors to detect different types of samples. To provide
precise results, the YL6500GC is equipped with a detector which has high linearity and reproducibility of
signal. Also, it has an accurate function which controls temperature to prevent sample from liquidizing and
to improve sensitivity.
For automation of gas sampling, valves can be installed separately for a gas sample injection. These can
be equipped up to four additionally with common inlets
Also, multi-positioning vales are available up to two for applications of various gas samples.
The YL6500 GC promotes the retention time of sample and the accuracy of experiments by improving
the precision and accuracy of temperature of column oven. The temperature of oven is controlled in a unit
of 1 ℃ from room temperature up to 450 ℃. If you want to operate the instrument below room
temperature, you have to install extra cooling equipment which uses liquid nitrogen or carbon dioxide.
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Detector
- Maximum no. of detector installation: three
- Data Acquisition Rate : 200 Hz
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Chapter 2. Installation
You have to check the environment for installation before opening the box of the YL6500 GC.
The YL6500 GC is approximately 605 mm width, 550 mm depth, and weighs 55 kg. Although you can
usually use ordinary experimental desk, you had better check whether it support the YL6500 GC or not.
To operate the YL6500 GC normally, it is recommended to maintain the indoor temperature between 15℃
and 25 ℃, and humidity between 50% and 60%.
The column oven of the YL6500 GC draws off warm air from the back side of the equipment. Therefore,
you should install the equipment away from a wall at least 30 cm, and keep something which can be
harmed by warm air away from the back side.
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There are following signs about safety on the surface of the equipment. Please, take the advice of
messages when you operate or repair the equipment.
When you open the cover of the equipment, it is safe not to turn it on.
You have to keep something which must not be heated such as wires, gas lines, and chemicals away
from the back side, because the oven exhausts hot air from the back side. Also, you must not touch the
hot inlets and detectors.
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2-2. Check
Firstly, check the condition of the box of equipment and then inspect the status of it. If you find any flaw,
feel free to contact us.
Secondly, check the Packing List attached on the box whether there are any missing items or not. If you
find out any missing, do not hesitate to contact us.
2-3. Power
The YL6500 GC is adjusted to be used in 220 VAC ( 5%), 60 Hz, and the consuming voltage is 3.5 KW. It
is recommended to install the Auto Voltage Regulator (AVR) – capacity 5.0 KW - in a place where the
change of voltage is severe.
You can provide the equipment with power and ground because the offered power cable contains the
ground line and plug also has ground. 어지
2-2-3. Ground
For safety, the IEC (the International Electro technical Commission) recommends to ground the
equipment. Therefore, you should check the connection of ground before installing the equipment. If there
is no ground line in a power socket, you have to connect the extra ground line to the ground part of a plug.
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1. Carrier gas
When selecting a TCD, you use helium as carrier gas and nitrogen in the case of analysis of hydrogen.
Also, when you select a FID, helium, nitrogen, or hydrogen is possible for carrier gas. But hydrogen is
often not used because explosion may occur. Therefore, when using both a TCD and FID, you have to
obtain helium and nitrogen. Besides, other detectors (ECD, NPD, FPD) usually use nitrogen and helium,
too. But you have to use optimal carrier gas when taking a special detector like PDD.
2. Purity of gas
Although there are some exceptions according to usage or detectors as the following table 2-1, you have
to use pure carrier gas normally above 5N(99.9995%)
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You have to use 1/8 inch metal tubes in outer diameter (O.D.) for all gases. If you use a plastic tube,
oxygen in air can infiltrate it and other impurities like plasticizer can harm a column and a detector. Also,
you must not use old tubes contaminated by oils because they pollute gas tubes connected to the
equipment.
1) Regulator
Use regulator suitable for the types of gas and shape or size of cylinder. If possible, use it having
CGA(Compressed Gas Association) numbers.
3) Oxygen Trap
Even a little oxygen in carrier gas can harm a column, especially a capillary column with very little
stationary phase and lower the performance of a EDC detector. Therefore, if selecting an ECD, be
sure to use an oxygen trap. This trap is installed next to a moisture trap.
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On/Off Valve : The On/Off Valve is not essential, but useful. You must install it to the outlet of매우연겨은 a
regulator.
Mmoisture trap : You need a moisture trap for carrier gas, and must install it with every detectors. Install it
Oxygen Trap : You need an oxygen trap for carrier gas. When using an ECD detector or a capillary
column, you must install it. Generally, it is essential for a packed column, too. Install it to the
outlet of a moisture trap.
Connect the tube for carrier gas to the back-right side of the YL6500 equipment, “CARRIER”. When
selecting FID as a detector, connect each tube for air or hydrogen to “AIR” or “HYDROGEN”. If using other
valves for gas sample, connect the tube for compressed air or nitrogen to “VALVE GAS”.
1) Connect all gas tubes. (Do not open the cylinder valve yet.)
2) Adjust the pressure controlling valve in order to make the second-order pressure gauge of the regulator
to zero.
3) Open the cylinder valve. If there is a opening and closing valve, open it, too.
4) Adjust the pressure controlling valve in order to make the second-order pressure gauge of the regulator
to about 50-70 psi.
5) Check gas leakage from the connection part of the regulator and the cylinder to the backside of the
YL6500 GC by using the bubbles.
6) When finding some leakage, tighten the connection part and check the leakage again.
7) See whether the pointer of the pressure gauge goes down or not when closing the outlet of GC and the
cylinder valve. If the pointer goes down at once, there is some leakage. Therefore, you must check the
leakage again.
8) If you can not find any leakage, continue to install the equipment.
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Chapter 3. Screen
The wide LCD screen conveys a lot of information at the same time. There are three main icons on
Home screen, which are [System], [GC], and [Display]. [System] icon is to set the system. [GC] icon is to
set parameters. [Display] icon is to show current status of GC.
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SYSTEM Screen
[System] screen is to check the basic information and environment setting of instrument, run the self-
diagnosis function, calibrate the temperature and flow rate, and control the other special functions. System
screen is configured with seven tab screens, and each tab screen can be displayed by tapping one of tabs
on the top.
GC Screen
[GC] screen is to set parameters. Each item screen is moved by tapping the top tabs, and parameters
are entered by the key pad. Oven, Injector, Detector, and Signal tabs are activated with the default and
Valve and Methanizer tabs are activated depending on whether these are installed or not.
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DISPLAY Screen
[Display] screen is to indicate the current status of GC. The current status is displayed at the upper left-
hand and right-hand. It displays [READY], [NOT READY], or [RUN] at the upper left-hand side depending
on the current status. When a special function is operated, it displays [POST RUN], [READY] [RUN], [GAS
SAVER], or [COLUMN COND] at the upper right-hand side. While an analysis is running, it displays an
oven temperature, a step for oven program, run time, and run time in progress. In the case of a repeat
analysis, it shows the number of total analysis and current analysis.
YL6500 GC can be installed up to three inlets and three detectors, and each is displayed as [FRONT],
[CENTER], [REAR] depending on the its position. You can see temperatures, flow rates, and signals for all
inlets and Detectors, and if tapping on one of inlets or detectors tab, it displays the temperature, flow rate,
and signal in order. Not installed inlets and detectors are deactivated.
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* Status message
Message Description
Not Ready Either an entered temperature or flow rate does not reach to set point.
Post Run When cleaning the column after finishing an oven program
Gas Saver Reducing the flow through a split vent during an analysis
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YL6500 GC
YL6500 GC has a key pad for entering settings and each function. There are twenty three keys on the
key pad and it is configured with numeric keys and menu keys which are located LCD screen below.
HOME
This key is used to move the initial screen consists of three icons [System], [GC] and [Display].
Ready Run
This key is used to be back to the initial parameter of split flow after an analysis is done.
If [Gas saver] mode is operated to capillary inlet, parameters return to initial status, but split flow retains
as saved in [Gas saver] mode in order to save the gas continuously. At this time, if pressing [Ready Run]
key, split flow is set to the initial value so that a split injection is performed normally.
ON / OFF
Makes each function activated or deactivated. It is used for turning on or off the each function.
START
This key is used to start the process of GC analysis. When injecting a sample manually, press the [Start]
key after an injection. If Autosampler is installed with GC, no need to press the [Start] key because
Autosampler sends a start signal automatically to GC.
STOP
This key is to used to stop the process of GC analysis. When pressing [Stop] key during an analysis, the
analysis stops then all parameters return to the initial state.
CANCEL
This key is used to delete all settings you entered.
ENTER
This key is used to enter the settings. It is not activated if pressing the [ENTER] key only. You need to
select [ON] key in order to its activation.
POWER
This [Power] key is used for turning on or off the LCD screen, not a power supply switch.
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YL6500 GC
YL6500 GC displays the current status of instrument by using three LEDs on the top of control panel.
[POWER] LED light indicates whether power is supplied or not, [READY] LED lights up when actual value
reaches to set point, and [RUN] LED light is on during the running.
POWER
[POWER] LED is turned on if the power is supplied to the instrument. If not, [POWER] LED is off.
READY
Once all of the conditions reach to set point then the equilibration time elapses, [READY] LED is on.
RUN
When pressing [Start]key , [RUN] LED is turned on, and an analysis is running.
Screen setting
When you enter parameters for items installed on your GC, select each item and enter desired value on
LCD screen by using a touch pen supplied with GC or touching softly on it with your finger.
Operating function
To operate a desired function, touch on a desired item`s tab then select [ON]. To stop the operation,
select [OFF].
Parameter entering
To enter parameters such as temperature or flow rate, touch on a screen you want to enter. Input
parameters in where cursor is on, using numeric keys and then press [Enter] key.
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3-2-1. Configuration
Enter the environment settings of GC system, for instance, the current date, time. IP Address, Port No.
and Password, Key Lock, Key beep, and Autosampler settings are set on this configuration screen.
Date
Enter the current date depending on your local date. The initial date is based on the delivery date from
the factory. It can be altered with a eight-digit. The format is YYYY/MM/DD.(Year/Month/Day)
Time
Enter the current time depending on your local time. The initial time is based on the delivery date from
the factory. It can be altered with a six-digit. The format is HOUR/MM/SS.(Hour/Minute/Second)
Port No.
Enter a Port No. The initial value is based on the delivery at factory.
Password
Enter a password of GC system. If selecting [ON] at Password option, a password configuration window
displays and enter your password with a four-digit on this window.
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YL6500 GC
Key Lock
[Key Lock] makes the Key function locked. If selecting [ON], keys do not work. Initial setting is [OFF].
Key Beep
[Key Beep] allows you to hear the beep sound when tapping on the screen. Initial setting is [ON].
3-2-2. Information
[Information] screen displays the basic information of your GC system such as model name, firmware
version, and what items are installed. Any parameter can not be entered on this screen.
If Valve is installed on GC, [NEXT] key is activated at the bottom and you can move to [Valve] screen with
this key to check the status of Valve.
Model
It is to indicate the Model name of GC
Version
It is to indicate a F/W Version which is the control type used in producing an equipment. If ROM version
is upgraded or downgraded, displayed version is changed automatically.
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YL6500 GC
Serial No
It is to indicate a serial number which is unique for each instrument. Users can not change arbitrarily this
settings.
Installed
It is to indicate the date when an instrument is delivered from the factory. Users can not change arbitrarily
this settings.
Cryogenic
It is to indicate whether or not Cryogenic option (LN 2 or CO2) is installed. If Cryogenic option is installed,
entering the below zero temperature is possible.
Autosampler
It is to indicate whether or not Autosampler is installed on GC. To check whether Autosampler is installed,
firstly turn on Autosampler prior to switching GC on.
Update
This function is used for updating GUI(Graphic User Interface) program, so users should be careful to
operate this function.
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YL6500 GC
Valve
It is used to check the type of valve, the number of port, and loop volume. If not installed, tabs are
deactivated.
Auxillary
It is used to check the temperature of Auxillary items. If Auxillary items (valve, methanizer) are not
installed, it indicates as [Not Installed].
3-2-3. Diagnosis
YL6500 GC has a self-diagnosis function. This self-diagnosis function is very useful to inspect the status
of instrument. Various functions are available on [Diagnosis] screen and these functions are to check oven,
APC, inlet and detector, and output for solenoid valves movement on Main board. Note that, this
procedure could affect serious problems to the system if an unqualified person performs.
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APC
APC self-diagnosis checks the function of APC controlling flow rate of inlet and detector. You may check
the function of Voltage, Leak, APC Sensor and APC valve on [APC] screen.
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Inlet
Inlet self-diagnosis checks the flow rate and temperature of installed inlets.
Oven
Oven self-diagnosis checks the function of oven. You may check the function of Voltage, Valve, Position
Valve, DA, Zero Crossing, and Temp. on [Oven] screen.
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Detector
Detector self-diagnosis checks the function of installed detectors. Checking option is different depending
on the type of detectors. You may check the function of ADC, Power, and Ignition ECD Reference Current
on [Detector] screen.
3-2-4. Calibration
This screen is to calibrate the temperature and flow rate for oven, injector, and detector. Displayed icon is
different depending on your GC`s configuration. You can move each item by tapping one of items you
want to calibrate.
<Caution>
This procedure should be performed very accurately. Therefore, the instrument
encounters serious problems if an unqualified person performs. This procedure can
be performed by only trained and qualified service engineers.
[Calibration] screen shows seven calibration items. You can select an item you want to calibrate among
seven items, which are Oven, Injector 1, Injector 2, Injector 3, Detector 1, Detector 2, Detector 3 by
touching each item. Note that, if you touch on [RESET] key, the calibration is not performed and then back
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Oven
The function of [Oven Calibration] is to calibrate the temperature. You can move each calibration option
with arrow keys at the bottom and touching tab buttons on the top. After completing the calibration, [END]
message is displayed. In case that an error occurs during calibration procedure, [Fail] message is
displayed and you need to perform again from the beginning. The current temperature of oven shows on
[Act] tab. To calibrate the temperature of oven, set the oven to a temperature of 100℃, then wait until the
temperature is stable. After stabilization, measure the actual temperature of oven using an approved
thermometer. Input settings for temperature on [Set] tab, then input measured temperature on [Measured]
tab. After setting these parameters, press [ON] key to perform the temperature calibration.
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Inlet
Calibrates the temperature, proportional valves and flow rate for inlet on [Inlet] tab. [Pressure Calib.]
function is added to Capillary inlet.
Temp
Calibrates the temperature of inlet. The current inlet temperature displays on [Act] tab. To
calibrate the temperature of inlet, set the inlet to a temperature of 100℃, then wait until the
temperature is stable. After stabilization, measure the actual temperature of inlet using an
approved thermometer. Input settings for temperature on [Set] tab, then input measured
temperature on [Measured] tab. After setting these parameters, press [ON] key to perform the
temperature calibration.
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Sensor Zero
The function of [Sensor Zero] is to perform zero adjustment for Flow sensor. This procedure
should be performed under condition of atmospheric pressure, no gas flow, and room temperature.
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Valve Calibration
The function of [Valve Calibration] is to calibrate valves installed on APC block. This procedure
should be performed under condition of gas flow and room temperature. To perform this procedure,
press [ON] key on the key pad. During this procedure, each voltage of Valve 1, Valve 2, and Valve
3 is displayed on the screen and calibrated automatically.
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Flow Calibration
Flow calibration should be performed by an approved flow meter and you have to keep this flow
in good condition carefully. Capillary inlet calibrates the flow rate of Purge and Split. Packed and
On-column inlets calibrate only flow rate of Column. Actual flow rate is displayed on [Act], and
input flow rate of Split and Purge then wait until flow rate of Purge and Split reaches to set point.
When flow rate is stable, measure actual flow rate using an approved flow meter. Input a
parameter for flow rate on [Set] tab, then input measured flow rate on [Measured] tab. After setting
these parameters, press [ON] key to perform flow calibration.
Pressure Calibration
The function of [Pressure Calib.] is to calibrate the pressure of Capillary inlet.
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Detector
Calibrates the temperature, proportional valves, and flow on [Detector] tab. The sort of used gas is
different depending on detector, therefore, firstly select the gas used for your detector then start to do
calibration procedure. All procedure is same with Injector section.
3-2-5. Special
This screen displays special functions for user convenience. The special function consists of 5 functions
and you can move by tapping [NEXT] arrow at the bottom.
Run Start
This is to run Auto repeat analysis function. You can set the number of running, run time, and cycle time.
No. of Run
It displays the number of running. If you set this number, you don‟t need to press the [Start] key
Run time
Set the running time for each analysis. You can not set this run time arbitrarily. The run time, which
Cycle time
Set the [Cycle time] for each run. Cycle time should be longer than Run time or same with it. GC
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Post Run
[POST RUN] function is to clean the inside of a column after finishing an analysis operated by an
oven program. You have to properly set treatment temperature in [Temp] tab and treatment time in
[Time] tab according to the kind and features of a column. If not use this function, set the treatment
time in [Time] tab to 0.0 min.
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.
Fig 3-22. Special function screen of YL6500 GC (Post Run)
Column Condition
When you need column conditioning and initialization of column because of installing a new column,
operating the GC without using it for a long time, or finding a peak tailing which is caused by impurities
that are absorbed in a column for long usage, you can use this function. [Rate], [Final Temp] and [Final
Time] tabs are activated when setting on [Column Condition].
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Remote Access
You can set functions which send a simple signal to operate external devices. You can set the time for
delaying a signal from an external device and that for starting an external event by sending a signal to an
external.
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YL6500 GC
YL6500 GC offers [Time control] function which enables you to operate your GC by a given time. A clock
inside of GC makes GC run according to the time control program. When tapping on [Time control] tab, a
table is displayed, and you can set DATE, TIME, and Function. You are able to make up to twenty steps.
Date
Enter the date when you will operate with a six-digit. The date is a YY/MM/DD format. (Year/Month/Day)
Time
Enter the time when you will operate with a six-digit number. The time is a HH/MM/SS format.
(Hour/Minute/Second) Entered times are classified automatically in chronological order.
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Function
Enter the function you want to operate automatically. If tapping on [Function] tab, you are able to select
necessary functions from the Function list.
Function List
Function Description
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3-2-7. Method
The function is to load all parameters as Method file you saved. The [Method] function lets you recall and
use all environment settings such as a temperature program, a flow program, parameters for a detector,
signal, a valve, etc. by saving them at a time in a method number. Therefore, you do not need to
remember all parameters for an analysis. Total 20 method files can be saved. The color of [Method] button
is changed depending on whether it is saved or not, and it is able to overwrite altered parameters into an
exist method file. If tapping on [RESET] key, all method files are deleted.
If touching one of method numbers, it shows as below screen whether it is saved or not. To save the
method file, tap on [SAVE], and to load a method file, tap on [LOAD]. If you want to close this screen, tap
on [CLOSE] at the upper right-hand.
3-3-1. Oven
There are 2 tabs which are [Config.] to set the basic environmental condition of oven and [Setting] to set
the analysis condition.
Config.
This is to set the basic environmental condition.
Maximum Temp
You can set a maximum oven temperature.
Equilib. Time
The Ready LED lights on when there is no change in set-up temperature within the Equilib. Time.
The Equilib. time setpoint can be 0.1 to 9999 minutes.
Cryogenic System
If you want to use a Cryogenic system, turn on this function and select one among LN2 and CO2.
Setting
This is to set up an analysis condition of oven. The current temperature is indicated in [Act]. Enter the
settable temperature into [Set]. Depending on Oven Mode, the oven program will be activated. You can
put the temperature ramping rate, setpoint temperature and specified period of time. (-) temperature can
be set when the Cryogenic System is ON. Temperature programming is available up to 25 ramps and the
maximum run time is 9,999 min.
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Temp.
Enter either the initial temp. or the temp for an isothermal run. To set temperature programming,
enter the settable temperature and press [ON].
Time
It‟s the specified period of time in the set temperature.
Rate
o
This is the ramping rate of temperature. The maximum ramping temp. is 100 C/min. When you
set the rate to 0.0, the temperature programming is not applied from the next step.
Final Temp.
It‟s the final temperature that is to be reached at the ramp rate.
Final Time
It‟s a specified period of time to hold the temperature at the final temperature.
Oven Mode
There are isothermal and program (temperature programming) modes. The ramp temperature
program is up to 25 steps and the maximum run time is 9,999 min.
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There are three tabs of Config. of Inlet and it‟s activated depending on the inlet location. The Inlet is
composed to two tabs which are Config. to set the basic environmental condition and Setting to se the
analysis condition. Purge Flow is set automatically to 3 ml/min.
Config.
Column Setup
Enter the installed column specification such as column length, inside diameter and film thickness.
Gas Saver
This function reduces the flow of carrier into the inlet and out the split vent after the injection is
complete to avoid unnecessary gas consumption. In this condition, the column flow rate and
pressure are maintained while split vent flows decreases. This is to be applied to the capillary inlet.
Time : Enter the time that Gas Saver starts based on run time.
Flow : Enter the split flow when Gas Saver function is on.
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Carrier Gas
There are 5 kinds gases to be selected as a carrier gas which are N2,He,H2,Ar and Ar/Me.
APC Mode
There are 4 column flow control modes(APC modes) which are Constant Flow, Constant Pressure,
Detector Connection
Setting
This is to set up an analysis condition of inlet. The current temperature, column flow and pressure of inlet
are indicated in [Act]. When you set APC mode to Programmed Flow or Programmed Pressure, you‟ll be
able to program the flow and pressure. Programmed Flow and Programmed Pressure can be set up to 5
steps. You can select parameters in Injection Mode and the screen configuration is changed depending on
Injection Mode.
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Temp.
Set the temperature of inlet.
Column Flow
Set the column flow. Settable flow range is 0.1~100 ml/min.
Velocity
This is to indicate the column flow to a velocity.
Split Ratio
This split ratio determines the injected sample amount which is injected into a column and the
amount which is drained into the split vent line. If you input a split ratio, the equipment controls Split
Flow and Total Flow automatically according to the ratio.
Injection Mode
- Split : A split injection method is generally used to inject small quantity of a sample into a
capillary column. It makes very small quantity reach at the column according to split ratio of the
injected sample.
- Splitless : A splitless injection method is suitable for a microanalysis of a solute which has high
boiling point and dissolved in a solvent having low boiling point. And the method is used when the
concentration of a sample is low. This method lets all sample go into a column during some time
and then takes the split injection type.
In a splitless mode, Split Ratio turns to Split on Time. This time(Unit : min) is the period of
operation in a splitless mode to a split mode. Setting this parameter to 0.0 turns the operation to a
split mode right after the start of analysis.
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Config.
Column Setup
Enter the installed column specification such as column length, inside diameter and film thickness.
Carrier Gas
There are 5 kinds gases to be selected as a carrier gas which are N 2,He,H2,Ar and Ar/Me.
APC Mode
There are 4 column flow control modes(APC modes) which are Constant Flow, Constant Pressure,
Detector Connection
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Setting
Temp.
Set the temperature of inlet.
Column Flow
Set the column flow. Settable flow range is 0.1~100 ml/min.
Pressure
This indicates the pressure at the column.
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Config.
Column Setup
Enter the installed column specification such as column length, inside diameter and film
thickness.
Carrier Gas
There are 5 kinds gases to be selected as a carrier gas which are N2,He,H2,Ar and Ar/Me.
APC Mode
There are 4 column flow control modes(APC modes) which are Constant Flow, Constant Pressure,
Detector Connection
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Setting
Temp.
Set the temperature of inlet.
Column Flow
Set the column flow. Settable flow range is 0.1~100 ml/min.
Pressure
This indicates the pressure at the column.
Temp. Mode
It‟s able to set a temperature programming for an on-column inlet. There are 3 modes available for
a temperature programming which are Isothermal, Program and Track Oven. In a Program Mode,
it‟s able to set a temperature programming up to 5 steps.
Config.
Lit offset
“Lit offset” is a standard value for acknowledging an ignition failure when “Auto ignition” function is
set. That is to say, when signal values are under a set value, the ignition is repeated. (Default : 5)
Delay Time
It is recommended to set a delay time to have enough time for the outside temperature of FID to
reach over 150℃ . If not, there could be some moisture inside of FID block even if FID temperature
already reached this point. Once FID reaches over 150℃, FID will start ignition after this time by
flowing an auxiliary gas.
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Ignite Flow
Set a flow rate of air. The default value is 100ml/min.
Ignite Temp
This is the temperature that FID can attempt the auto ignition. The auto ignition only works after reaching
this temperature.
Makeup Gas
Select a Makeup Gas which is mostly a same gas as a carrier gas. Pressing button changes the
gas type. There are 5 kinds gases to be selected as a carrier gas which are N2,He,H2,Ar and
Ar/Methane.
Connection
Select the inlet that is connected to a detector.
Signal Autozero
When this is set to ON, a signal starts from „0‟ in an analysis.
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Setting
Temp.
Set a temperature of detector. It is recommended to set over 150 ˚C for FID to be ignited.
Air
Settable flow rate range of air is 0~ 500ml/min. Mostly, the air flow rate is set in 300~400 ml/min.
H2
Settable flow rate range of hydrogen is 0~100mL/min. Mostly, the H2 flow rate is set in 20~40 ml/min.
Mkup Gas
Settable flow rate range of Mkup gas is 0~100ml/min. Mostly, the Mkup gas flow rate is set in 20~40
ml/min. This is same as the carrier gas.
Electrometer
This has to be ON to get a signal from a detector.
Auto Ignition
When you set auto ignition function at a FID, ignition starts automatically. Firstly, select [ON] at
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[Electrometer] and [Auto Ignition] after setting temperature of a FID. Then, air and hydrogen flow
automatically and auxiliary gas is ready to flow. When temperature of a detector reaches a setting
value, mixture of air and hydrogen flow and ignition start after [Ignition Delay Time] elapses.
If ignition fails even with trials more than 15 times, you can see an error message which tells you to
check the system and auto ignition stops.
Signal Range
Set a signal acquisition range. Settable range is 0.0 to 1000000.
Makeup Gas
Select a Makeup Gas which is mostly a same gas as a carrier gas. Pressing button changes the
gas type. There are 5 kinds gases to be selected as a carrier gas which are N 2,He,H2,Ar and
Ar/Methane.
Connection
Signal Autozero
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Setting
Temp.
Set a temperature of detector.
Ref. Flow
Set the flow rate that is toward the cell flowed standard current.
Sense
This parameter is to change the sensitivity of TCD by changing the current toward to the cell.
Filament
This is to supply a power to a filament inside of TCD. Check there flows a carrier gas before
pressing ON. It is able to turn ON only if the flow rate of sample/reference is over 10ml/min.
When there is a current flowing to the TCD cell, it can sense the signal.
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Polarity
This function changes the polarity direction of a peak of a TCD. You can use this function when
analyzing the component which has larger thermal conductivity than a carrier gas. You can change
the direction of a peak only when the above component emerges and return the direction to the
original (+) again.
If “Polarity Change” is “OFF”, the polarity is always “+”. If you want to change polarity, press ON at
“Polarity Change”.
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Config.
Makeup Gas
Select a Makeup Gas which is mostly a same gas as a carrier gas. Pressing button changes the gas
type. There are 5 kinds gases to be selected as a carrier gas which are N 2,He,H2,Ar and Ar/Methane.
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Setting
Temp.
Set a temperature of detector. It is recommended to set over 150 ˚C for FID to be ignited.
Mkup Gas
Settable flow rate range of Mkup gas is 0~100ml/min. Mostly, the Mkup gas flow rate is set in 20~40
ml/min. This is same as the carrier gas.
Electrometer
This has to be ON to get a signal from a detector.
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3-2-8. Signal
Config.
Zero
The detector signal is red from some point after subtracting this Zero value.
Range
Set a signal acquisition range. Settable range is 0.0 to 1000000.
Signal Change
When this is ON, the detector output can be changed.
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3-2-9. Valve
Config.
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Type
Select the type of valve installed on GC. There are 2 types of valve which are LSV and GSV.
Port
Set the no. or port.
Volume
Set the size of sample loop.
Conn.
3-2-10. Methanizer
Temp.
Set a temperature of a methizer.
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3-2-11. Auxillary
Config.
Max Temp.
Set a maximum temperature of Auxiliary.
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Setting
Temp.
Set a temperature of Auxiliary.
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4-1. Introduction
Inlets
In the YL6500 GC, you can install up to 3 inlets as shown in the above figure and maximum inlet
temperature is 450℃. We assume in this manual that the nearest one to the front side is as Front, the
middle one is as Center, and the back one is as Rear. There are two inlet systems. One is an inlet for a
packed column and the other is an inlet for a capillary column as an inlet system. If necessary, you can
install an on-column inlet.
There are many ways to inject a sample into a chromatography column. An inlet system is determined by
components of a sample and the type of a used chromatography column. The role of an inlet is to change
a phase of all or parts of a sample into a gas phase in order to inject it into a chromatography column.
Generally, inlet temperature is set about 20℃ higher than temperature to volatilize a sample component
which has the highest temperature to be volatilized and also about 20~50℃ higher than column
temperature. To inject a sample, you can use a micro syringe through a septum which is at the end of an
inlet. Although a septum has an ability to prevent a sample from leaking, you have to change it after using
it many times. Also, an injection of a sample is made in a moment because a peak width should be short
to have a good result of a quantitative analysis by letting a peak be separated well from an adjacent peak.
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The YL6500 GC has the APC (Advanced Pneumatic Control) systems which control all gas flowing
electronically to have high accuracy and convenience. The APC can be installed up to 6 at inlets,
detectors, etc., and enables all inlets to be set in terms of flow and column pressure.
0 - 400ml/min N2,
Total Flow rate range 100 mL
1 - 800ml/min H2 or He
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Generally, a column having the inside diameter less than 750m is used at a capillary column inlet, and
the inside diameter of used columns is typically less than 320m. Since a capillary column has smaller
surface area than a packed column, even a 1l sample may harm the column. Therefore, you have to
inject 1l or less than. To inject this small quantity, you can use a split injection method which lets only
portion of a sample go into a column at an inlet itself. When the concentration of a sample component is
very low, you can use a splitless injection method which reconcentrates the sample during some time and
then the sample goes into a column. You can control these methods by using the keypad and LCD screen
on the front side.
A split injection method is generally used to inject small quantity of a sample into a capillary column. It
makes very small quantity reach at the column according to split ratio of the injected sample. Generally,
the maximum sample quantity which does not carry an overload at a inside diameter 0.25mm WCOT (Wall
Coated Open Tubular) column is 10-50ng per the component of the sample. That for a WCOT column
which has large inside diameter and a SCOT (Support Coated Open Tubular) column is 1-10μg per the
component of the sample. Therefore, high split ratio (50:1 ~ 500:1) is suitable for a WCOT column having
high analysis ability, low split ratio (10:1 ~ 50:1) is proper for a WCOT column which has big sample
capacity and large inside diameter and a SCOT column.
A sample is injected into the inside heating region through a septum. Carrier gas will mix the vaporized
sample well at an inlet having high temperature. At a split point, some of a sample go into a
chromatography column and the rest is pushed out through a split vent line. You can control the flow which
flows in a column and the flow of a split vent by using LCD screen and number keys on the key pad. The
purge vent is kept 3ml/min constantly. The split ratio is defined as the following.
When analyzing a harmful sample, you can connect the end of a split vent to a fume hood or a trap. For a
split of a sample in the case of split injection method, there may be quantitative errors when some
components of a sample are not fully vaporized. And if inlet temperature is too high, there may be loss of
components due to chemical decomposition or new chemicals which are not in an original sample may
happen. A split injection method is not suitable for a microanalysis because most of a sample is wasted.
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A splitless injection method is suitable for a microanalysis of a solute which has high boiling point and
dissolved in a solvent having low boiling point. And the method is used when the concentration of a
sample is low. This method lets all sample go into a column during some time and then takes the split
injection type.
A capillary column inlet is composed of an inlet for injecting a sample and the APC which controls the
flow of the inlet as the following figure.
There are basically two glass inserts for a capillary column inlet in the YL6500 GC. One is the cup type
for a split and the other is the straight type for a splitless. Be sure to use them according to their uses.
Split / Splitless
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The APC(Advanced Pneumatic Control) means a system which controls gas stream electronically. The
system controls the flow of gas used for a detector as well as the carrier gas used in the YL6500 GC. The
APC uses electronic valves and sensors which control the flow of gas. There are four control modes -
Constant Flow, Constant Pressure, Programmed Flow, and Programmed Pressure – for controlling the
flow.
The constant flow mode keeps flow rate constant during an analysis. Generally, if gas temperature will be
changed, gas pressure or flow rate of gas also varies. Therefore, this mode will change the gas pressure
to keep flow rate constant when temperature varies.
The constant pressure mode keeps the pressure acting on a column constant during an analysis.
Therefore, this mode will change flow rate somewhat when column temperature varies.
You can program the flow rate of carrier gas electronically in an analysis process by using the ramped
flow mode as you program the temperature of an oven in terms of time in a GC analysis. The
programming step is available up to five steps.
The ramped pressure mode can electronically program the gas pressure which acts on a column during
an analysis. Also, the programming step is available up to five steps.
The gas saver function prevents gas from wasting by reducing the flow through a split vent during an
analysis after injection of a sample. Although the flow through a split vent is reduced, the pressure acted
on a column and the flow through the column remain constant. You can use this function in every setting
(Split/Splitless/pulsed split/pulsed splitless) and manage on the LCD screen.
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After starting “Run” by injection of a sample, the split flow remains constant during the indicated time in
this function and then the gas saver function starts. In the case of the Splitless, if the “Saver Time” is
smaller than the “Split On Time”, the value is not valid.
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The YL6500 GC has three inlets. Generally, we designed a capillary column is for the [Front] or [Center]
and a packed column is for the [Rear]. Therefore, we are assuming that the inlet is connected with a
capillary column in the Front and the other inlet is connected with a packed column in the Center.
In order to control the flow of carrier gas, you must choose the type of carrier gases, the environment of
APC system, and then other details.
- Choose the type of carrier gas at the bottom. The displayed type of carrier gas is changed
whenever touching on it.
- Choose a control method for the flow on APC Mode.
- Select the detector location connected to the inlet on Detector conn.
You can choose the kind of carrier gas by touching on Carrier gas tab.
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You can set the dimension of column, and the position of injector and detector connected to the column.
Input the length, diameter, and film thickness of a used column by touching on tabs and number keys on
keypad, and then press [Enter] key. You have to input these values because flow rate is determined by
length and diameter in a capillary column.
2) Choosing detector
Select the detector location connected to the inlet on Detector conn. by touching on this icon repeatedly
until it displays the desired type.
You have to make a function setting of APC before setting flow or pressure of carrier gas. You may
choose a control method for flow on APC Mode by touching on this icon.
You can choose four control modes for the carrier gas flow by touching on APC Mode icon.
The modes are determined by selecting one among four modes (Const Flow, Const Press, Ramped Flow,
Ramped Press). The carrier gas flow is changed by temperature. If you select the mode of Const Flow, the
pressure will be adjusted automatically and the rate of flow will be remained at a certain value. In the
mode of Const Press, the rate of flow will be a little changed according to temperature because the
pressure of the column is adjusted constantly. If using a packed column, you can select only the mode of
If you select Ramped Flow mode, the mode screen contains entries for setting up the program. With this
mode, you can control the flow of carrier gas according to time. You begin with entering the initial flow rate
(InitFlow), initial flow quantity, and initial time (InitTime) on the key screen. The unit of flow rate is ml/min,
and time is expressed in min. In the next step, you can input the value of „Rate 1” in order to change the
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Enter the desired value of the first step flow rate (Final Flow1) and the remained time reaching the flow
rate. If desired more, enter the second value into the second row. Repeatedly, you can set upto 5 steps.
With the mode of “Ramped Press”, you can set up the program similarly. But if choosing a packed
column, you cannot do this.
prevents the waste of carrier gas by reducing the quantity of flow through the Split Vent during the runs. If
you select this function, the column pressure and quantity of flow is kept constantly even though the
Select [ON] on Gas Saver, and input the values of time and quantity of carrier gas that flow through the
Split Vent during the function.
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1) Temp
Set the temperature parameter of the inlet. To determine the temperature of the inlet, firstly touch on Set
tab and input desired value (the unit is C) using number keys then press Enter key. The maximum
temperature is 450 C, and you can set the temperature in units of 1 C. But you can set up it until 400 C
Press [ON] key on key pad to heat it until the set point. Then you can see the set point instead of “OFF”.
If you want to change the temperature during the heating period, just put the desired value and press
ENTER】.
2) Injection Mode
In this step, you can determine the way of injecting a sample for the inlet of a capillary. There are two
sample injection modes – Split and Splitless. Choose one mode between of them by pressing Injection
Mode icon.
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3) Pressure
You can set up the column pressure in the case of Constant Pressure mode when determining the
function of APC. The input range is between 0.01psi and 100 psi. To set up the pressure value, just input
the desired value and press [ENTER] key regardless of “OFF‟ or a certain value.
4) Col Flow
You can determine the flow rate through the column in the case of using a packed column or the
Constant Flow mode in the function of APC. The rate range is between 100ml/min and 0.1ml/min. To set
the value, just put the desired value and press [Enter] key without regard to the case of “OFF” or a certain
value.
b. Split Flow
This determines flow rate which flows to an exit of an inlet after being splitted. If you change a split
flow, a split ratio and a total flow are changed according to this because a column flow is a fixed
value.
7) Total Flow
A total flow is a value which is added a column flow, a split flow, and a purge flow (exited to a septum). If
you change a total flow, a split ratio and a split flow is changed because a column flow is fixed.
When selecting a packed inlet, you need to input only inlet temperature and flow rate of carrier gas as the
following window shown by using number keys.
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5-1. Oven
An oven is a device which improves accuracy and confidence of an analysis result by controlling column
temperature exactly for an analysis. The standards of the YL6500 GC are followings.
An oven controls temperature using a heater and a fan when a flap door at the back side of the oven is
opened or closed. It cools up to +5℃ higher than room temperature without extra cooling device. The
oven temperature is measured by using a platinum RTD (resistant temperature detector). If analyzing a
sample under room temperature, you need extra cooling device such as liquid nitrogen ( -80℃ ) or dry ice
( -50℃ ). Temperature programming is available up to 25 steps and maximum running time is 9999min. In
order to open the oven door, just push a button on the right-down side of the oven door. This oven is
designed to stop to operate an oven fan and a heater when the oven door is opened during running in
order to protect a user and the equipment.
In order to operate the oven, firstly you have to make environment setting and operating condition for it
by tapping on LCD screen and using numeric keys on key pad.
To access the following screen, tap on [GC] icon at [Home] display then touch on [Config.] tab of [Oven]
item. In order to input parameters, tap on each tab, input parameters by using numeric keys then press
[Enter] key.
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The items about environment setting of an oven are shown in the following table.
Coolant LN2/Co2 To select the type of gas used for cryogenic option.
After tapping on [Setting] tab and selecting [Oven mode] as [Program], enter the oven parameters for
program mode on the following window.
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On the above window, The temperature on [Set] tab indicates an initial temperature of program mode.
Initially, it displays “OFF”. In order to set the initial temperature, tap on [Set] tab and enter parameter with
numeric keys and then press [ON] key. As soon as pressing [ON] key, the oven starts to heat immediately.
That is to say, if a temperature value is shown on the [Set] tab, the oven heater is operating.
“InitTime” means the time (min) which goes from pressing [Start] key in order to operate a ramping
program to starting ramping. After this time, the ramping program starts. (In the case of an isothermal
analysis, this is running time for an analysis.)
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By pressing [Enter] key after inputting each value at [Rate], [Final Temp], and [Final Time] in the first row,
you can make the first step ramping program. If tapping on a down arrow, you can see the second step
ramping program window. You can make the ramping program as the first step program. If you input 0.0 at
[Rate] in the second row, the other step ramping programs will be invalid as well as the second step
th
program. If you continue, you can make the ramping program until the 25 step.
o
Temp on [Set] tap C Initial temperature or temperature during an isothermal analysis
Time which goes during maintaining initial temperature for an
Time minute isothermal analysis,
Or run time for an isothermal analysis
Ramping rate of an oven at each step, Maximum effective ramping
o o
Rate C/min rate is 100 C/min.
If you input 0.0, the next steps will be invalid from the step.
o Final temperature which is reached by heating at the former ramping
Final Temp C
rate.
Final Time minute Time which maintains the final temperature
At first, an oven is at initial temperature. But, if you press [Start] key, a ramping program will start. When
ramping program goes, the error range between measured temperature and set program is less than 0.5
o
C.
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The following figure is a graph about changes in terms of time and temperature when temperature
programming runs.
Explanation of the following figure “ti” is the time which is set at the above “ init time” and “t1” and “t2” are
times which go to each “final temp1” and “final temp2” at “Rate1” and “Rate2”.
Also, “tf1” and “tf2” mean each “final time1” and “final time2” which go at final temperature.
Ti = initial Temp, Tf1= final Temp 1, Tf2= final Temp 2
Tf
Final
2 Temp2
Temp(T)
Rate2
Tf
Final
1 Temp1
Rate1
Ti
Initial Temp
ti t1 tf1 t2 tf2
Time (t)
The following is [Post run] screen. To access this function, tap on [System] icon at [Home] display, touch
on [Special] tab and then tap on [NEXT] arrow at the bottom until this screen is displayed.
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You can use the [POST RUN] function to clean the inside of a column after finishing analysis according
to an oven program. You have to properly set treatment temperature on [Temp] tab and treatment time on
[Time] tab according to the kind and features of a column. If you will not use this function, set the
treatment time [Time] as 0.0.
You can use [Ready Run] key for the case which the functions such as [Gas saver] and [Splitless] are set
in a program for a capillary column inlet. If these functions are set, you have to set the flow conditions for
operating these as initial values after finishing a GC program.
If you want to use this function, set the flow condition as initial value for operating a sample analysis
program by pressing [Ready Run] key after finishing a sample analysis. And then, inject a sample. If
[Ready Run] runs, you can see [Ready Run] message on [Display] screen.
You can operate the instrument automatically without pressing [Ready Run] key after every analysis is
done by the following procedure. If tapping [Special] tab at [System], you can see the following window.
Then, if you select [Auto Readyrun] to [On], the equipment operates automatically.
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5-2. Column
A column plays an important role in separating components in a sample. It is installed between an inlet
and a detector. You have to check out a fitting, and a liner, an adapter, and an insert which are used at an
inlet, and a detector to install a column. Especially, in the case of a 1/4 inch glass column, you have to use
the column according to standards because the column is chosen according to the distance between an
inlet and a detector.
Columns are divided into several parts according to what they are made of. Even though they are made
of same materials, they are also divided into several parts according to purposes of usage and kinds of
stationary phase.
Columns are divided roughly into packed columns and capillary columns. A packed column is packed
with something and a capillary column is a column whose inside is coated with stationary phase. Columns
are divided into GSC and GLC according to the status of materials which is packed in or coated in a
column.
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1) Packed Column
A packed column is made of stainless steel, glass, nickel, etc.. the average of length is about 6~20 feet.
Normally, the outside diameter (O.D) is 1/8 inch, 3/16 inch, or 1/4 inch and the inside of diameter (I.D) is
2mm ~ 4mm. Stationary phase which is packed in this column is a solid itself or a solid on which
nonvolatile liquid is coated. Generally, resolution is low. The packed stationary phases are methyl silicon,
molecular sieves, , porous polymer, etc. and other special materials are used for the packed stationary
phase.
2) Capillary Column
Generally, the inside diameter (I.D) of a capillary column is about 0.1-0.53mm, and very thin film is
coated on the inside of the column. Since pressure depression of gas according to length is not very
large in the case of a capillary column, the column can be very long (10-100m). Therefore, the theoretical
plate is greatly large. But, the quantity of a sample which can be injected is very small. A capillary column
is mainly made of fused silica and also unusually made of stainless steel.
3) GSC
This column is packed with solid stationary phase and mainly used for separating inorganic gas or
hydrocarbon having low molecular weight by absorption at room temperature. The used stationary phase
is charcoal, silica Gel, zeolite, molecular Sieve, porous polymer, etc..
4) GLC
If stationary phase is liquid, liquid is coated on solid support, which is packed in a column. The quantity of
liquid should be enough to be coated on the solid support. But, too much reduce efficiency of the column.
Also, since retention time is proportion to the quantity of liquid, small quantity enable you to analyze a
sample quickly. Liquid have to resolve components of a sample and have different partition ratio according
to the components. Also, it have to be nonvolatile and be stable so that it does not react with a sample
chemically.
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5-2-2 Fitting
You need some kinds of fittings to install a column at GC. The following table summarizes features of
typical fittings.
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A liner and an adapter are installed at the inside of an oven and are used to connect a column with an
inlet and a detector. An insert is used only for an inlet. You have to install these before installing a column.
b. Place the insert into a liner for a packed column inlet with making the
trumpet part on the end of the insert up.
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1) Put a nut and a ferrule into a column. If you put an O-ring before putting a nut, it prevents the
column from damage.
2) Slide the column into an inlet and a detector fully.
3) Take down about 1-2mm and tighten a column nut by hand.
4) Use a wrench to tighten the column nut just to prevent leakage.
5) Check leakage by using bubbles. If necessary, tighten it more.
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Since mostly a new column contains volatile pollution which is absorbed in the atmosphere, you have to
eliminate these to obtain a stable base line. In the initialization of a column, operate the equipment with
connecting the column to an inlet, but do not connect it to a detector. When doing this, close the detector
with a cap or a plug.
Chapter 6. Detector
6-1. Introduction
You can install two detectors in the YL6500 GC. Generally, a Flame Ionization Detector (FID) and a
Thermal Conductivity Detector (TCD) are used. In this manual, we assume you have installed a FID at
[Front] and a TCD at [Rear].
Besides, you can install a Nitrogen Phosphorous Detector (NPD) which has good sensitivity especially
for nitrogen or phosphorous, an Electron Capture Detector (ECD) which captures high energy electrons
63
(-rays) produced by using a radioactive isotope ( Ni), a Pulsed Discharge Detector (PDD), a Flame
Photometric Detector (FPD), etc. according to analysis purposes. More details are explained in the
supplement.
Generally, detectors are divided into universal detectors and selective detectors. If a detector can detect
all components like a TCD, it is a universal detector. On the other hand, selective detectors are detectors
which can detect only certain components according to use and the above all detectors except for a TCD
belong to them.
Besides, synthetic detectors such as AED(Atomic Emission Detector), FT-IRD, MS(Mass Analyzer), etc.
are used.
TCD
FID
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+
Therefore, a FID detects signals in proportion to the numbers of carbon atoms. CHO ions which are
produced by flames carry current to an anode above the flame. Therefore, current which flow from a
cathode under the flame to an anode are measured by a recorder. A FID can detect all organic
compounds, but volatile compounds and gas such as O 2, CO2, H2O, NH3, etc. can not be detected. A FID
can not detect or rarely detects the following compounds.
6-2-1. Sensitivity
2
Detector‟s response to an organic compound is proportion to sample‟s weight and sensitivity is about 10
times higher than it of a TCD. Generally, you may use N 2 as carrier gas (You can also use He gas.). But
when you use a capillary column, it is recommended to use H 2 or He gas as carrier gas. Also, you can
have good detection result when using N2 gas as support gas to increase flow velocity when a sample
goes into a detector.
Sensitivity of a detector responses to the ratio of H and carrier gas(N2) very sensitively. The ratio should
be in 1:7~10. It is recommended to adjust ratio to obtain what has the best sensitivity because the best
ratio may be different according to equipments. When you use a capillary column, flow rate of carrier gas
is the sum of flow rate in the column and that of auxiliary gas.
In a FID, hydrogen and air are used to make flames. Generally, it is recommended to adjust the ratio to
1 : 7 or 1 : 10, flow rate of hydrogen to 30-40 ml/min, and that of air to 300-400 ml/min to make ignition
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easily. Although flow rate of hydrogen is the fact which greatly influences ignition and sensitivity of a
detector, that of air is less sensitive than that of hydrogen and so
enough air to make ignition is OK. Flow rate of air is enough when it
is about 7-10 times of that of hydrogen. For example, it is no matter
that flow rate of air is a bit large when concentration of a sample is
thick, but it is recommended that it of air is small when the
concentration is thin. There are some cases not to be ignited well
when flow rate of carrier gas is large. Then, increase flow rate of
hydrogen a little.
1) FID Jet
You have to replace a FID Jet according to the type of a used column (a packed column or a capillary
column). If you are going to use a packed column after using a capillary column, you have to change a jet.
A 0.011 inch jet shows the greatest sensitivity of a detector when a capillary column is used. When using
a 0.018 inch jet for a packed column, you have to pay attention to use it because flames of a FID may be
distinguished.
2) Collector
A collector is a place where ions which are ionized at a FID come together. It is located around the upper
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of a jet and is made of metal. The ions which are gathered at this are carried to a FID board and produce
signals.
3) Ignitor
An ignitor is heating wires to ignite a FID. The end of this is connected with a power of electricity and the
other end is grounded to the FID body. If current flow through the heating lines, the wires produce heat
and ignite fuel gas.
You have to make an environment setting of the detector before using a FID. If tapping on [Config.] tab of
[Front] detector, you can see the following window.
The detail items are explained in the following table. To input a value, press [Enter] key after entering
each parameter. If you want to change the sort of makeup gas, press [Makup Gas] tab until it displays a
desired gas.
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He
Select the kind of auxiliary gas. Generally, use the same kind of
H2
Makup Gas carrier gas as a make-up gas. If tapping [Makup Gas] tab, you can
N2
choose the kind of gas used for FID.
Ar/CH4
[Lit offset] is a standard value for acknowledging an ignition failure
0.0~9999
Lit offset when “Auto ignition” function is set. That is to say, when signal
(counts)
values are under a set value, the ignition is repeated. (Default : 5)
It is recommended to have delay time for raising temperature of
outside before making ignition because moisture may be produced
at a FID block when ignition is made before that of outside is not
Delay Time 0~999(min)
high enough. Although temperature of a FID is above 150℃, that of
outside may not be so high. That is to say, after spending delay time
after reaching 150℃, ignition starts by flowing auxiliary gas.
Set the flow rate for air when starting the ignition. Generally, set
Ignite Flow
100ml/min.
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Set necessary parameters on [Setting] of [Det] tab where FID is positioned. To input a value, tap on each
tab, input parameters using numeric keys and press [Enter] then [On] key. If you want to change
parameters during the operation, just tap on a tab you want to change and input parameters using numeric
keys then press [Enter] key.
Auto Ignition ON/OFF You can turn on/off the auto ignition function.
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Auto ignition function : When you set auto ignition function at a FID, ignition starts automatically.
Firstly, select [ON] at [Electrometer] and [Auto Ignition] after setting temperature
of a FID. Then, air and hydrogen flow automatically and auxiliary gas is ready to
flow. When temperature of a detector reaches a setting value, mixture of air and
hydrogen flow and ignition start after [Ignition Delay Time] elapses.
If ignition is confirmed (Auto confirm), the ignition process stops and ready
status for an analysis starts. If you want to confirm the ignition, just check the
signal on [Signal] tab by pressing a down arrow key.
If you install a capillary column, flow make-up gas (MkUp gas) properly.
If ignition fails even with trials more than 15 times, you can see an error
message which tells you to check the system and auto ignition stops.
6-3-1. Introduction
A thermal conductivity detector (TCD) is included in a universal detector because it can detect all
materials which have different thermal conductivity from that of carrier gas. Thermal conductivity is a
measure how well a material carries heat according to temperature difference. The higher thermal
conductivity, the faster heat moves.
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It is recommended that the difference of thermal conductivity between a sample component and carrier
gas is big because response of a detector result from the change of thermal conductivity of flow.
Generally, hydrogen (H2) and helium (He) are used as carrier gas because their thermal conductivities are
big. Although hydrogen have the best sensitivity because it has the largest thermal conductivity, you have
to be careful to use it due to danger of explosion. Therefore, helium is used as carrier gas mostly.
Although nitrogen and argon are used as carrier gas, they are used only for a special analysis because
they are used in low sensitivity for avoiding damages of a filament and shows low response to most
materials. You have to be careful to treat a filament of a TCD because it is apt to be damaged by air or
oxygen.
Make an environment setting on the following window by tapping on [Config.] of [Det] tab where TCD is
positioned.
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Select the kind of make-up gas(Mkup/REF) by taping on [Makup] tap. Be sure to choose the same kind
with carrier gas. Every time you press this tab, one of the available gases(He, N2, Ar, H2, 5%CH4/Ar) is
displayed.
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2) Temperature setting
You have to set enough temperature of a detector for a sample which comes from a column not to be
condensed. But, a TCD has better sensitivity when temperature of the detector is low.
You have to make each flow rate be more than 10ml/min at least. If flow rate is less than 10ml/min, the
power of a filament is cut off automatically to protect a TCD cell. And you have to make each flow rate of
carrier gas through a reference column and an analysis column be same to obtain stable signals when
analyzing a sample. Therefore, refer to the flow rate value from the inlet connected to TCD.
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5) Polarity change
This function changes the polarity direction of a peak of a TCD. You can use this function when analyzing
the component which has larger thermal conductivity than that of carrier gas. You can change the direction
of a peak only when the above component emerges and return the direction to the orignal(+) again.
If [Polarity] is selected to [OFF], the polarity is always “+”. If you want to change polarity, select [ON] at
[Polarity] tab.
If you want to change initial status of polarity, press [NEXT] arrow key on [Setting] tap and choose Initial
State to “-” or “+”.
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For example, If you input 1.5 min in the first [Time] tap, 1min in the second [Time] tap and select initial
state to “+”, polarity changes to negative(-) after 1.5min (Time1) then the it changes to positive(+) again
after 1.0min(Time2). If a value of [Time] tab is 0.0, polarity will not change.
Here, if you make “Value” be “ON”, signals which go to a terminal are shown up. And you can see the
signal values.
If you see the back side of the equipment, you will see terminals which carry signals of a detector to the
outer and they are labeled “DA 1”, “DA 2” and “DA 3”. Although normally signals of detector-1 (Front) are
carried to the “DA 1” terminal, detector-2 (Center) are carried to the “DA 2” terminal, and detector-2 (Rear)
are carried to the “DA 3” terminal, you can change the order by signal conversion function.
This function makes the “DA 1” terminal select signals of detector-1, detector-2 and detector-3
electronically. But it does not make component which is separated in column-1 enter detector-1,
detector-2 and detector-3 selectively.
If you want to change the output of signals, tap on [Setting] at [Signal] tab then you can see the following
window. You can select a detector position which accepts signals initially and input signal conversion time.
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If you input a value in the first [Time] tab, a detector in parentheses will be changed to other detector
position which is different from an initial detector. For example, signals come from a TCD, but they come
from a FID after 4.5 minutes. If you again input a value in the second [Time] tab, the detector in
parentheses will be changed to the initial detector (TCD). In this way, you can make signal conversion of a
detector up to 5 steps.
If you want to remove a signal conversion time which is inputted already, just input 0.0min to [Time] tab.
For example, if you want to input again from the beginning, just input 0.0 in the first [Time] tab.
You can not change the time while program is running.
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7-1. Introduction
You can inject gas sample into an inlet directly with a syringe in
Gas Chromatography. But, this method has not good
reproducibility. Therefore, you need an extra injection device. You
can use a gas sampling valve to inject gas sample. The device is
installed at the fore part of a column. The maximum valve number
is 4 in the YL 6500 GC, and the program is possible up to 30.
Injected gas sample is contained in a sampling loop and then, it is carried by carrier gas into an analysis
column to be analyzed. You need a valve which can change the path of gas variously for the process such
as containing a sample in a loop, carrying it through carrier gas, etc.. Generally, 6-ports or 10-ports valves
are frequently used as a valve which treats gas sample. Although the connecting method is various
according to the purpose, basically a valve for a capillary column is installed when GC is delivered.
When you treat the gas which is condensed at room temperature due to its high boiling point, you have to
raise temperature of a valve before using. Since maximum temperature and pressure are different
according to valves, you have to properly choose one according to samples. There are some methods
such as a manual method, an air actuated, an electric actuated, and a micro-electric actuated method to
operate valves. Here, explanation is done on the basis of an air actuated method.
2-position air actuator is attached at the top to open or close a valve for gas sample. An air actuator is
operated by air or nitrogen and the proper pressure is 40-80 psi.
Basically, the capacity of an installed sample loop for injecting a sample is 250μL. Therefore, if you want
others having different capacity, you have to order them.
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If tapping on [Config.] at [Valve] tab, you can see the window for environment setting for a valve.
You can choose either [LSV] (Liquid sampling valve) or [GSV] (Gas sampling valve) by tapping on [Type]
icon.
Enter the number of port and the volume of sample loop size, and select the inlet position where valve is
connected by tapping on [Conn.] tab.
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We have explained the basic principle and the operating method of the equipment for each part in the
above chapters. But we will explain the operation procedure synthetically to operate the equipment
actually in this chapter. You have to check prerequisites and necessary parts for operating the equipment
well. After this, you can operate the equipment easily by knowing the following checklist and simple
procedure for operating it.
The YL6500 GC needs stable power source. Therefore, it has an auto voltage regulator. Moreover, if
you use an extra power device for an electricity failure, you can prevent experimental results from
vanishing due to the power failure. Since the maximum spending power is 3.5 kW, it is recommended to
use the auto voltage controller whose output voltage is 220V and maximum power is 5kW.
Confirm that the power cable is connected correctly and GC is connected with the data system rightly.
Refer to chapter 2 (Installation) for method connecting the cables.
Select proper carrier gas used for GC according to the type of an used detector and its purity has to be
high (more than 99.995%). If necessary, install traps for eliminating moisture or oxygen and a refiner
additionally. Also, prepare extra auxiliary gases. (Refer to chapter 2.)
When you analyze a sample in gas chromatography, the most important part is an analyzing column. The
columns differ according to components which is analyzed. You can choose the column by using a
reference or an experiment. After selecting a column, install a column and take an initialization step before
using it. Refer to chapter. 5 for the column initialization.
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∙ Set the column specification : Enter the length, inside diameter and the film thickness of the column
∙ Select a carrier gas at “Carrier Gas”.
∙ Select the flow control modes : Constant flow/pressure, Programmed flow/pressure
6. Input the pressure or flow rate of a column.
If you want to use a TCD, enter a temperature only after a checking column flow rate and a reference
cell flow rate are on to a TCD.
8. Input a flow rate and necessary factors of a detector
FID: Autoignition, Electrometer ON
TCD: Set a flow rate of REF/Mkup gas – Filament ON
9. Stabilize a column.
Check the signals to be stabilized after it reaches to the setting a temperature.
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8. Enter a temperature of inlet, detector and oven. The detector temperature should be more than 150℃
to be ignited.
9. Initialize and stabilize a column
10. Turn on the electrometer and the auto ignition of a FID, and set make-up gas (Mkup gas) when
installing a capillary column.
11. Check signals after confirming the ignition of the system.
12. Run a chromatography data system to display the acquisition window.
13. Enter acquisition conditions to the CDS
14. Press【START】button right after injecting a sample
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8-3-3.ECD analysis
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It‟s required to eliminate impurities remained in a column after finishing an analysis. Therefore, perform
“Post run” process by increasing a temperature of oven to clean out the column.
After all process, turn off the instrument by the following procedure.
6. Separate the column from the detector after temperature of an oven is below 50 ℃ and that of a
detector is below 150 ℃.
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Chapter 9. Maintenance
When using the equipment, sometimes you are faced with the need to maintain and repair it. This
chapter describes maintenance procedures and requirements of YL6500 GC.
9-1. Introduction
9-1-1. Maintenance list
Maintenance lists with time to replace are summarized in the following table.
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Since the YL6500 GC controls temperature of an oven, an inlet, and a detector by electricity, be careful to
manage the heating and electric parts.
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A trap for eliminating impurities of carrier gas is connected from a carrier gas cylinder to the equipment.
Generally, a moisture trap is connected to the exit of the carrier gas cylinder and an oxygen trap is
connected from the equipment to the moisture trap.
1) Moisture Trap
A S-shaped moisture trap is used to eliminate a trace level of moisture which is in carrier gas. The
moisture is harmful to the mobile phase of a column when the equipment is operating in high temperature
and induce the deterioration of a detector like an ECD. This moisture trap is generally packed with
“Molecular Sieve 5A”. If carrier gas contain very big contamination which is difficult to be absorbed on
“Molecular Sieve 5A”, you can use “Molecular Sieve 13X” or “Activated Charcol” as an absorber.
This moisture trap can be used again by conditioning in an oven. For conditioning, connect the moisture
trap to an inlet after closing the exit of a detector in the same method for column conditioning. Then,
switch on the oven at 350℃ for at least 3 hours with flowing N2 or He at 60ml/min. If you want to pack the
trap again, clean it after removing the old packing materials it with new “Molecular Sieve 5A”.
2) Oxygen Trap
An oxygen trap is used to eliminate a little oxygen which is in carrier gas. The oxygen harm a capillary
column. Moreover, when using a high sensitive detector like an ECD, you have to use the trap because
oxygen is a hindrance in the ECD. But this trap can not be used again after conditioning and have to be
replaced.
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9-2. Inlet
This is to maintain a carrier gas system connected to the back of the equipment, an inlet for a packed
column (a packed inlet), and that for a capillary column (a capillary inlet).
3. Replacing a septum
Generally, you have to replace a septum every 30~50 injections. Especially, if you use it at 250℃above,
you have to change it more frequently. When replacing, close the carrier gas cylinder. To replace a
septum, input a septum to "Septum Retainer Nut" and tighten it a little by hand. And then, raise a
temperature and tighten it again.
If the used septum is coated with Teflon, install it with making the coated surface be toward downside of
an inlet.
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4. Cleaning an inlet
Remove a column and a liner after eliminating the septum retainer nut and the septa while the inlet
temperature is to be room temperature. The liner contains a glass insert. If the glass insert is
contaminated, wash it with chromic acid first and then in order of distilled water, methanol and acetone.
After that, dry it up fully at 150℃.
Clean the liner which is removed from the inlet with 0.1% nitric acid and wash it with water. And then,
make ultrasonic cleaning with methanol.
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4. Cleaning an inlet
A capillary inlet is designed to slide an insert into it. Although you do not have to clean the inside of the
inlet fully, it is very important to clean the insert of the inlet. Therefore, you have to clean or replace the
insert at least every 3 months. If necessary, clean up the inlet. You have to disconnect carrier gas
connection tube which is connected already and remove the insert which is installed at “Insert Retaining
Assembly” to clean up the inlet. Then, clean the inlet with a proper brush. If necessary, wash the inlet with
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neutral detergents or methanol. After cleaning, dry up the inside of the inlet fully by flowing carrier gas with
connecting carrier gas connection tube.
If you want to pack the insert again, put the treated glass wool in the nozzle part inside the insert and
pack “10% OV-1 on 80/100 mesh Chromosorb WHP” in it. And then, put the glass wool in it again. Since
about 2 inch syringe has to be used, keep about 35mm space when packing.
Check the O-ring before puting the insert in the inlet. If there is no wrong, install an O-ring at the 5 mm
upside of the insert and input the insert in the inlet. And then, slide it as down as possible.
9-3. Oven
The oven is a device which controls temperature of a column. (Refer to chapter 5.) If the oven gets
organic materials or dirts in it, there will be soots or dirty marks since its temperature is very high.
Therefore, when you do not use it, clean it using a dried rag with methanol, aceton, etc.. You can replace
heaters and sensors in the heating parts including the oven whenever necessary.(You had better ask the
service department to replace them.
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3. Column conditioning
Contamination of a column is mainly induced by remants which is not volatilized. Even a new column has
volatile pollutants which is absorbed from air. Especially, the column which is leaved alone for a long time
without colsing the end of it, is sure to have pollutants. Therefore, you have to make column conditioning
before using it.
Since colunm conditioning differs according to the kinds of columns, refer to data obtained when buying a
column. Column conditioning means the thermal conditioning which is happened while carrier gas is
flowing through the column. You can make the column conditioning by the following procedure.
Select “COLUMN CONDITION” among items after pressing【SPECIAL】in the GC control screen.
Do not connect a column with a detector before column conditioning and close the input of the detector
with a cap to prevent it from contamination.
For most columns, Set initial temperature to 50℃ and initial time to 30min. And then, Set the maximum
temperature depending the kinds of the columns.
Do not raise temperature of an oven more than the maximum tempearture of the column. This is because
such action decreases the life time of the column and damages the column rapidly. Especially, if using a
capillary column, you must not raise the temperature rapidly and have to use it under the maximum
temperature of column. Set “Fin Temp” under the maximum temperature of the column and raise the
temperature at about 3℃/min. slowly for column conditioning.
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9-4. Detector
1. Replacing a jet
If using a FID, you have to change a jet depending on the kind of the used column (a packed column and
a capillary column)
1. You have to install a jet before installing a column. If you replace a column, you have to change a jet
before installing the column.
2. It‟s essential to use a 0.011 in. jet for a capillary column. If you use it for a packed column, the ignited
flame may be distinguished.
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2. Cleaning
A collector and a jet may be contaminated by white silica or black carbon materials from a column. These
contaminators decrease the sensitivity and induce “Noise” and “Spike” phenomena. Therefore, you have
to clean them to remove these materials.
Turn off the detector and adjust the temperature to be room temperature. Close all cylinders for gases
used for the detector. Open the upper-cover of the equipment.
You can clean them as the following procedure.
ⓐ Switch off the equipment and disconnect the power cable from the electric outlet.
ⓑ Remove a signal connector from a FID
body. .
ⓒ Disconnect the connector which is
connected with the equipment and the ignitor.
ⓓ Loosen the collector nut by hand.
Fig 9-6. FID Jet
ⓔ Check the gasket whether it is damaged or
not by inspecting the bottom of the collectror mount after removing 4 screws holding it.
ⓕ Disconnect the collector body, the upper collector insulator, and the low collector insulator which are
installed in the collectror mount.
ⓖ Spin counterclockwise the jet installed in the FID body with a jet driver and pull out it with a pincette.
ⓗ Clean the upside of the FID body with solvent, compressed air, or nitrogen.
ⓘ Check the damage of the jet and replace it with a new jet which is proper for the column. Then,
tighten it with a jet driver.
※ Reference ※
ⓙ Assemble the collector. The high collector insulator which the bottom part is long is located under the
collector body. The low collector insulator is flat and a round shape and is located above the collector.
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※ Reference ※
If the signal shows “1,000,000”, generally there is water which is produced
by air and hydrogen in the collector. Therefore, remove water. This is
because air and hydrogen flow in the low temperature of the detector. Open
the cylinders of air and hydrogen always when the temperature of the
detector is more than 150℃, and ignite then.
3. Operating an ignitor
If the ignition of a detector is not stable, you can hardly see the red flames at the exit of the detector. For
this case, you have to check the ignitor or the related circuit. If “Ignition failure” happens more than 3 times
when you operate the auto ignition function, you can think that the ignitor may be cut.
Firstly, measure the resistance between the terminal of the middle cable of the ignitor and the case with
the DVM. If the measured resistance is infinity, replace the ignitor because it is cut.
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4. Ignition trouble
If the following facts are observed, you can conclude that the jet is damaged. The facts are that the flow
rate of the detector is correct, that there is no gas leakage, that the flow rate of carrier gas is right, that the
ignitor runs well during ignition, and that the detector is not contaminated.
※ Reference ※
If you have ignition failure when using He as carrier gas, it is because the flow
rate of carrier gas which is added with AUX gas. In this case, decrease the flow
rate of carrier gas which is added with AUX gas as low as possible. And if the flow
rate of carrier gas is high, increase the flow rate of hydrogen a little.
If you can not find any outside damage of jet, the damage is the jet‟s inside break which is produeced by
tigthening it too tightly. Therfore, you have to replace it. If ignition failures keep on happening in spite of
changing the jet, the problem is due to the detector‟s inside damage which is produced by tightening the
jet heavily. In this case, you have to replace the detector.
When you use a TCD, it is very important to protect the filament which is made of tungsten-rhenium. Be
sure to keep it from oxygen. And since the sensitivity is high when temperature is low, you have to use it
under low temperature.
When using the TCD, you may fine the movement of a baseline, the incrase of noises, the unexpected
peaks, etc. This phenomenon may be caused by a sample or the packed materials of a column which
enter into the TCD and contaminate it. In this case, you have to make the thermal cleaning which is known
also as “bakeout”. For the bakeout, make sure that there are no leakages of carrier gas or contaminations
of each inlet and detector.
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For the TCD, if a filament is cut, you have to replace the whole TCD block. If you can find “OVER
CURRENT” when using the TCD, firstly make the value of “SENSE” be smaller than the current value. If
“OVER CURRENT” keeps on happening in spite of the smaller values, you have to check both the board
and the cell. If “OVER CURRENT” is not shown when decreasing the value of【TCD SENSE】, you have
to adjust only VR2 of the board. If the filament of the TCD is cut, “OVER CURRENT” is generally shown
on the detector‟s screen. In this case, it happens whatever the value of 【TCD SENSE】is. For this, just
measure the resistance of the TCD cell. Here, you can know the method which tells how to measure and
check the TCD status.
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